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Acetone → HCID 22621002, 화합물

HRID 430429
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HRID 430429 반응식
[CH3:1]I.[CH3:3][C:4]1[CH:12]=[CH:11]C(C(O)=O)=[C:6]([NH:13][S:14]([CH3:17])(=[O:16])=[O:15])[CH:5]=1.[C:18](=[O:21])([O-])[O-].[K+].[K+].C[C:25]([CH3:27])=[O:26]>>[CH3:3][C:4]1[CH:12]=[CH:11][C:27]([C:25]([O:21][CH3:18])=[O:26])=[C:6]([N:13]([CH3:1])[S:14]([CH3:17])(=[O:15])=[O:16])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 22620944HCID 22620944, 화합물

생성물 1

HCID 22621002HCID 22621002, 화합물

실험 절차

Methyl iodide (22.0 ml) was added to a stirred suspension of 4-methyl-2-(N-methylsulphonylamino)benzoic acid (8.0 g) and anhydrous potassium carbonate (24.2 g) in acetone and the mixture was stirred and heated at reflux overnight. The mixture was cooled and filtered and the filtrate was evaporated to dryness. The residue was dissolved in dichloromethane and washed with aqueous sodium bicarbonate solution, water, dried (magnesium sulphate) and filtered. The filtrate was evaporated to dryness to give methyl 4-methyl-2-(N-methyl-N-methylsulphonylamino)benzoate (8.36 g) as a cream solid, m.p. 100-103° C.

후처리

  1. temperatureheated
  2. temperatureat reflux overnight
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. customthe filtrate was evaporated to dryness
  6. dissolutionThe residue was dissolved in dichloromethane
  7. washwashed with aqueous sodium bicarbonate solution, water
  8. dry with materialdried (magnesium sulphate)
  9. filtrationfiltered
  10. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-9bea601e4f6d4f1cae3f909694faf4ac
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06323155B1

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